Synthesis and crystal structural study of ternary molybdate NaMg3In(MoO4)5

We have synthesized single crystals of a temary molybdate NaMg₃In(MoO₄)₅ and cam'ed out an X-ray structural study (a KM-4 automatic difiactometer, MoK, radiation, 4503 F, R = 0.047). The triclinic unit cell dimensions are a = 7.0476(7), b = 17.935(2), c = 6.9849(7)Å, = 87.650(9), = 100.980(8), = 92.510(9)°, V= 865.5(2) A³, Z = 2, and space group P^–1. The crystal structure involves MoO₄ tetrahedra and (Mg, In)0₆ octahedra forming a three-dimensional framework with Na atoms located in its cavities. The compound melts at 990°C with decomposition.Institute of Inorganic Chemistry, Siberian Branch, Russian Academy of Sciences. Institute of Physics, Siberian Branch, Russian Academy of Sciences. Buryatian Institute of Natural Sciences, Siberian Branch, Russian Academy of Sciences. Translated fromZhurnal Strukturnoi Khimii, Vol. 34, No. 5, pp. 147–151, September–October, 1993.Translated by T. Yudanova     

Features of the atomic and electronic structure of the new nonlinear optical crystal KAlFPO4

A precision x-ray diffraction investigation of the crystal structure and the electron density of a single crystal of KAlFPO₄ has been carried out. Partial disordering of the K⁺ ions along a 2₁ axis has been discovered. According to the maps of the deformation electron density in cross sections of the principal anionic polyhedrons in the structure, the Al–O, Al–F, and P–O bonds have a partially covalent character, and in the last case there is also a component.D. I. Mendeleev Moscow Chemical-Engineering Institute. Institute of Crystallography, Academy of Sciences of the USSR. A. N. Nesmeyanov Institute of Organometallic Compounds, Academy of Sciences of the USSR. Translated from Zhurnal Strukturnoi Khimii, Vol. 32, No. 2, pp. 103–109, March–April, 1991.     

E and Z stereoisomers of compounds of the phthalide series

The stereospecific position of the H⁴ proton in the PMR spectra of 3-benzyl-idenephthalides identifies unambiguously the E and Z isomers in a mixture. The IR spectra of off-planar deformation vibrations of the C=C bond in the 990–970 cm^–1 region have strong absorption bands, assigned to the E and Z isomers. The strong short-wave band (260 nm) for 3-benzylidenephthalides, having only one benzene ring in the indan moiety, suggests the presence of the E form (=28,000). The long-wave absorption band at 390–430 nm belongs to the Z isomers (=21,000–31,000). 3-Benzylidenephthalides which have no carbonyl groups in their molecules, show fluorescence (_f1=540–560 nm in EtOH).N. N. Semenov Institute of Chemical Physics, Russian Academy of Sciences, 117977 Moscow. Translated from Izvestiya Akademii Nauk, Seriya Khimicheskaya, No. 2, pp. 309–314, February, 1992.     

Synthesis of derivatives of pentopyranic acid

N⁴-Benzoylcytosine 1-(methyl 2,3,4-tri-O-acetyl--D-glucopyranosiduronate) has been obtained with a yield of 70% by the glycosylation of the trimethylsilyl derivative of N⁴-benzoylcytosine with methyl 1,2,3,4-tetra-O-acetyl--D-glucopyranuronate in the presence of three equivalents of SnCl₄ as condensing agent. Cytosine 1-(-D-glucopyranosiduronamide) (IV) — the amide of pentopyranic acid — has been synthesized in practically quantitative yield by the ammonolysis of the nucleoside (I).Peat Institute, Academy of Sciences of the Belorussian SSR, Minsk. Institute of Bioorganic Chemistry, Academy of Sciences of the Belorussian SSR, Minsk. Translated from Khimiya Prirodnykh Soedinenii, No. 5, pp. 617–619, September–October, 1983.     

Obtusinin — A new coumarin fromHaplophyllum obtusifolium

The epigeal part ofHaplophyllum obtusifolium collected in Ustyurt has yielded -sitosterol, isofraxetin, and a new coumarin — obtusinin — with the composition C₁₅H₁₈O₆, mp 135–137°C (methanol), [] _D ²⁰ +140.9° (c 0.44; chloroform). The structure of obtusinin has been established on the basis of the results of a study of UV, IR, PMR, and mass spectra and also of some chemical transformations (hydrolysis, acetylation).Institute of the Chemistry of Plant Substances, Academy of Sciences of the Uzbek SSR, Tashkent. Combined Institute of Natural Sciences of the Karakalpak Branch, Academy of Sciences of the Uzbek SSR, Nukus. Translated from Khimiya Prirodnykh Soedinenii, No. 3, pp. 328–330, May–June, 1980.     

A chemical study of plants of the Mongolian flora lariside — A new scopoletin glycoside fromSalsola laricifolia

A new coumarin glycoside lariside — C₂₁H₂₆O₁₃, mp 155–156°C (from methanol) — has been isolated from the epigeal part ofSalsola laricifolia Turcz. et Litw. On the basis of acid hydrolysis and spectral characteristics the structure of lariside has been established as 7-[O--D-apiofuranosyl-(1 2)--D-glucopyranosyloxy]-6-methoxy-2H-1-benzopyran-2-one.Institute of Chemistry, Academy of Sciences of the Mongolian Peoples' Republic, Ultan-Bator. Institute of the Chemistry of Plant Substances, Academy of Sciences of the Uzbek SSR, Tashkent. Translated from Khimiya Prirodnykh Soedinenii, No. 3, pp. 288–291, May–June, 1986.     

Berberis alkaloids. XXI. Intebrine — A new N-benzylisoquinoline alkaloid from Berberis integerrima

A new N-benzylisoquinoline alkaloid — intebrine, with the composition C₂₀H₁₉NO₇ — has been isolated fromBerberis integerrima Bunge. The spatial structure of intebrine has been reliably determined by the x-ray structural method (diffractometer, CuK radiation, 972 reflections, direct method, R=0.048). Its chemical behavior, spectral characteristics, and mass-spectrometric fragmentation under electrom impact have been studied.Andizhan State Medical Institute. Institute of the Chemistry of Plant Substances, Uzbekistan Republic Academy of Sciences, Tashkent. Translated from Khimiya Prirodnykh Soedeninii, No. 1, pp. 65–70, January–February, 1993.     

Template synthesiS: Geometrical and electronic structures of the Fe nitrosyl complex formed by bis(S-methylisothiosemicarbazone)-2,4-pentandione

Sodium acetylacetonate reacts with S-metliylisothiosemicarbazidium nitrate and Fe(NO₃)₃ · 9H₂O in ethanol to make [Fe(HL)NO]NO₃, in which H₃L is bis(S-methyl-isothiosemicarbazone)-2,4-puntandione. The [Fe(HL)NO]⁺ cation has a square pyramidal structure with the HL^2- arranged around the central ion in the basal plane and the nitrogen atom of the NO group in the apical position, with the iron atom diverging from the plane of the base of the pyramid by 0.477 Å. The FeN0 moiety has a linear structure (FeNO = l72.7°). XRD, IR, and Mössbauer spectroscopy have been combined with calculations on the electronic structure to demonstrate that the Fe-NO bond is covalent.Chemical Institute, Academy of Sciences of Moldavian SSR. Applied Physics Institute, Academy of Sciences of the Moldavian SSR. Kishinev. Institute of Crystallography, Academy of Sciences of the USSR. Kurnakov Institute for General and Inorganic Chemistry, Academy of Sciences of the USSR, Moscow. Translated from Teoreticheskaya i Éksperimental'naya Khimiya, Vol. 27, No, 3, pp. 376–381, May–June, 1991. Original article submitted February 18, 1991.